固相萃取-气相色谱-质谱法测定化妆品中20种邻苯二甲酸酯  

GC-MS Determination of 20 Phthalates in Cosmetics by Separation with Solid Phase Extraction

作　　者：林钰镓 王小兵 于海英 李俊婕 高文超 刘莹 

机构地区：[1]山东省食品药品检验研究院,济南250101

出　　处：《理化检验（化学分册）》2016年第9期1031-1035,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重大科学仪器设备开发专项基金(2012YQ180132)

摘　　要：提出了同时测定化妆品中20种邻苯二甲酸酯类化合物的固相萃取(SPE)-气相色谱-质谱法(GC-MS)。不含油脂和含油脂的化妆品样品分别以正己烷和乙腈为溶剂作超声固相萃取,使其所含邻苯二甲酸酯类化合物溶于有机相中。萃取液经Cleanert PAE30006-C柱净化,所得净化后溶液进行气相色谱-质谱(GC-MS)分析。质谱分析中采用电子轰击正离子模式(EI+)和选择离子监测(SIM)模式,用外标法定量。20种邻苯二甲酸脂类化合物的质量浓度在0.1~10mg·L^(-1)范围内与峰面积呈线性关系,检出限(3S/N)在0.13~1.04 mg·kg^(-1)之间,样品加标回收率在79.2%~123%之间,相对标准偏差(n=6)在1.7%~12%之间。A method for GC-MS determination of 20 phthalate esters in cosmetics was proposed by separation with solid phase extraction. Samples of cosmetics were treated ultrasonically by SIDE with n-hexane as solvent for samples containing no oil and fat, and with acetonitrile as solvent for samples containing oil and fat, to extract the phthalate compounds into the solvent. The extract obtained was then purified by passing through Cleanert PAE30006 C column. The purified solution was used for OC-MS analysis. The modes of EI＋ and SIM were adopted in MS, and external standard method was used for quantification. Linear relationships between values of peak area and mass concentration of the 20 phthalates were found in the range of 0. 1- 10 mg·L^-1, with detection limits （3S/N） in the range of 0.13-1.04 mg·L^-1. Values of recovery obtained by standard addition method were in the range of 79. 2%-123%, with RSDs （n=6） in the range of 1.7%-12%.

关 键 词：气相色谱-质谱法 邻苯二甲酸酯 化妆品 固相萃取 

分 类 号：O657.63[理学—分析化学]